반응 #10351

반응 방정식

4-Amino-6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-pyrimidine

DBU

ethyl-sulfamoylchloride

→

ethyl sulfamic acid-[6-chloro-5-(o-methoxy-phenoxy)-2-(4-pyridyl)-pyrimidin-4-yl]-amide

용매

DCM

THF

반응 조건

후처리

1. 1
   기타The solvent was evaporated
2. 2
   workup.ADDITIONWater and a 10% solution of citric acid were added
3. 3
   추출followed by extraction with EtOAc and DCM
4. 4
   건조The combined organic layers were dried over sodium sulfate
5. 5
   기타the solvent was evaporated under reduced pressure
6. 6
   기타After purification of the residue by chromatography over silicagel with EtOAc/methanol/ammonia=4:1:0.5

실험 절차

4-Amino-6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-pyrimidine (100 mg) was dissolved in THF (5 ml) and DCM (5 ml). DBU (46 mg) and DMAP (37 mg) were added followed by the addition of ethyl-sulfamoylchloride (prepared from ethylamine hydrochloride and sulfuryl chloride). The mixture was stirred for 12 h at r.t. The solvent was evaporated. Water and a 10% solution of citric acid were added followed by extraction with EtOAc and DCM. The combined organic layers were dried over sodium sulfate and the solvent was evaporated under reduced pressure. After purification of the residue by chromatography over silicagel with EtOAc/methanol/ammonia=4:1:0.5, ethyl sulfamic acid-[6-chloro-5-(o-methoxy-phenoxy)-2-(4-pyridyl)-pyrimidin-4-yl]-amide (10 mg) was obtained. tR=4.31 min, (LC); [M+H]+=436.14 (ES+).

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